CN108689703B - Lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics and preparation method thereof - Google Patents
Lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics and preparation method thereof Download PDFInfo
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- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 20
- 238000000498 ball milling Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 12
- 238000003801 milling Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 3
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 2
- 238000004321 preservation Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 5
- 238000009768 microwave sintering Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 4
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a leadless ferroelectric ceramic material with giant dielectric constant and electric regulation characteristic and a preparation method thereof, wherein the ceramic material comprises the following components: (1-x)BaTi0.90Sn0.10O3‑xCa2LaMn2O7(ii) a WhereinxRepresents a mole fraction of 0.01<x<0.2. Wherein BaTi0.90Sn0.10O3And Ca2LaMn2O7The lead-free ferroelectric ceramic is separately synthesized by a solid-phase synthesis reaction method, and then a special small-scale hybrid complex structure is formed by mixing and once microwave sintering, so that the giant dielectric constant and the dielectric constant external field adjustable characteristic are generated, and the properties exceed all reported lead-free ferroelectric ceramics at present. The product has giant dielectric constant, electric regulation characteristic and dielectric constant measured experimentallyr~105The dielectric property can be regulated to 98%, the performance is stable, the cost is low, and the method is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a lead-free ferroelectric ceramic material for a capacitor and an electric tuning capacitor, in particular to a lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics and a preparation method thereof.
Background
The dielectric constant is a measure of the ability of a material to increase the capacitance of a capacitor relative to vacuum. The dielectric constant increases with increasing molecular dipole moment and polarizability. In recent decades, integration, miniaturization and high speed of electronic components have been the main driving force for the development of microelectronic technology, and high dielectric constant materials are the core materials of electronic components such as Dynamic Random Access Memories (DRAMs) and Multilayer ceramic capacitors (MLCCs). The giant dielectric constant ceramic material can further break through the bottleneck of miniaturization/microminiaturization and high-performance development of large-capacity capacitors and electronic elements, and is receiving wide attention.
Electric field tunable dielectric materials have gained considerable attention and research due to their important applications in components such as electrically tunable oscillators, electrically tunable filters, and phase shifters. Electric field tunable dielectric materials require as high a dielectric constant as possible for electric field tunability while also having as low a dielectric loss as possible, typically expressed in terms of dielectric tunability and figure of merit (dielectric tunability loss). The nonlinearity of the dielectric property of the ferroelectric material can realize frequency and phase agility, the nonlinearity is realized by utilizing the adjustable characteristic of an external field of dielectric constant, additional accessory elements and complex circuits are not needed, and the miniaturization is facilitated.
BaTiO3The base ferroelectric material has large dielectric constant and dielectric constant external field adjustable characteristic, but at present BaTiO3The giant dielectric properties of the base ceramics have been rarely reported.
Disclosure of Invention
The invention aims to provide an ABO3Perovskite structure with giant dielectric constant and external field adjustable dielectric constant BaTiO3The lead-free ferroelectric ceramic material is prepared by perovskite-structured ferroelectric BaTi0.90Sn0.10O3And Ca of Ruddlesden-Popper structure2LaMn2O7The ceramic material has stable performance and low cost.
The invention relates to a lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics, which comprises the following components:
(1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7(ii) a WhereinxRepresents a mole fraction of 0.01<x<0.2；
Wherein BaTi0.90Sn0.10O3And Ca2LaMn2O7The lead-free ferroelectric ceramic is separately synthesized by a solid-phase synthesis method, and then a special small-scale hybrid complex structure is formed by mixing and one-time microwave sintering, so that the giant dielectric constant and the dielectric constant external field adjustable characteristic are generated, and the properties exceed all reported lead-free ferroelectric ceramics at present.
The preparation method of the lead-free ferroelectric ceramic material with giant dielectric constant and electrically adjustable characteristic adopts a solid-phase synthesis method and combines microwave sintering to form a special hybrid structure, and comprises the following steps:
(1) according to BaTi0.90Sn0.10O3Respectively weighing and analyzing pure raw material BaCO according to the stoichiometric ratio3、SnO2And TiO2Putting the mixture into a ball milling tank, taking zirconia as a milling ball and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 24 hours, separating the milling ball, drying the raw materials at 60 ℃, and then preserving the heat for 2 hours in a high-alumina crucible at 1200 ℃ to synthesize BaTi in advance0.90Sn0.10O3Powder;
(2) according to Ca2LaMn2O7Respectively weighing CaCO as a raw material for analysis3、La2O3And MnO2Putting the raw materials into a ball milling tank, taking zirconium oxide as a milling ball and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 24 hours, separating the milling ball, drying the raw materials at 60 ℃, and then preserving the heat for 2 hours in a high-aluminum crucible at 1300 ℃ to synthesize Ca in advance2LaMn2O7Powder;
(3) the synthesized BaTi0.90Sn0.10O3Powder and Ca2LaMn2O7Powder according to (1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7(whereinxRepresents a mole fraction of 0.01<x<0.2) stoichiometric batching;
(4) ball-milling the raw materials prepared in the step (3) for 15 hours by using absolute ethyl alcohol as a medium, drying, adding 5% PVA (polyvinyl alcohol) for granulation, and carrying out cold isostatic pressing under the pressure of 150 Mpa;
(5) rapidly sintering the raw materials formed in the step (4) by adopting microwave, preserving heat for 30 minutes at 1400 ℃, and sintering into porcelain; the sintered sample is processed into a sheet with smooth two sides, and the two-side silver-plated electrode is prepared into the lead-free ferroelectric ceramic material with giant dielectric constant and electric regulation characteristics.
The lead-free ferroelectric ceramic material prepared by the invention has the dielectric constant measured by experimentsr~105The dielectric can be adjusted to 98%, and the dielectric constant-adjustable ceramic material has the characteristics of giant dielectric constant and dielectric constant external field adjustability, is stable in product performance, low in cost, green and environment-friendly, simple in preparation method and suitable for large-scale industrial production.
Drawings
FIG. 1 is a graph showing the giant dielectric constant and the dielectric constant external field tunable characteristic of the lead-free ferroelectric ceramic material according to the example.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited thereto.
Example 1
A lead-free ferroelectric ceramic material with giant dielectric constant and electrically adjustable characteristics comprises the following components: (1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7WhereinxThe number of the molecular weight is expressed as a mole fraction, x=0.02。
the preparation method of the ceramic material comprises the following specific steps:
(1) according to BaTi0.90Sn0.10O3Respectively weighing and analyzing pure raw material BaCO according to the stoichiometric ratio3、SnO2And TiO2Putting the mixture into a ball milling tank, taking zirconia as a milling ball and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 24 hours, separating the milling ball, drying the raw materials at 60 ℃, and then preserving the heat for 2 hours in a high-alumina crucible at 1200 ℃ to synthesize BaTi in advance0.90Sn0.10O3Powder;
(2) according to Ca2LaMn2O7Chemical meterWeighing CaCO as analytically pure raw material3、La2O3And MnO2Putting the raw materials into a ball milling tank, taking zirconium oxide as a milling ball and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 24 hours, separating the milling ball, drying the raw materials at 60 ℃, and then preserving the heat for 2 hours in a high-aluminum crucible at 1300 ℃ to synthesize Ca in advance2LaMn2O7Powder;
(3) the synthesized BaTi0.90Sn0.10O3Powder and Ca2LaMn2O7Powder according to (1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7(whereinxThe number of the molecular weight is expressed as a mole fraction,x=0.02) stoichiometric compounding;
(4) ball-milling the raw materials prepared in the step (3) for 15 hours by using absolute ethyl alcohol as a medium, drying, adding 5% of PVA (polyvinyl alcohol) for granulation, and carrying out cold isostatic pressing at 150 Mpa;
(5) rapidly sintering the raw materials formed in the step (4) by adopting microwave, preserving heat for 30 minutes at 1400 ℃, and sintering into porcelain; the sintered sample is processed into a sheet with smooth two sides, and the two-side silver-plated electrode is prepared into the lead-free ferroelectric ceramic material with giant dielectric constant and electric regulation characteristics.
Example 2
A lead-free ferroelectric ceramic material with giant dielectric constant and electrically adjustable characteristics comprises the following components: (1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7WhereinxThe number of the molecular weight is expressed as a mole fraction, x=0.05；
the preparation method is the same as that of example 1.
Example 3
A lead-free ferroelectric ceramic material with giant dielectric constant and electrically adjustable characteristics comprises the following components: (1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7WhereinxThe number of the molecular weight is expressed as a mole fraction, x=0.12；
the preparation method is the same as that of example 1.
The giant dielectric constant and the external field tunable dielectric constant characteristics of the ceramic materials prepared in examples 1 to 3 are shown in FIG. 1.
Dielectric property measurements for the ceramic materials prepared in examples 1-3 are shown in the following table:
the contents of the present invention will be further clarified by the examples given above, but they are not intended to limit the present invention.
Claims (2)
1. A leadless ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics is characterized in that: the ceramic material comprises the following components: (1-x)BaTi0.90Sn0.10O3-xCa2LaMn2O7(ii) a WhereinxRepresents a mole fraction of 0.01<x<0.2; wherein BaTi0.90Sn0.10O3And Ca2LaMn2O7The materials are separately synthesized by a solid-phase synthesis method, and then are mixed and sintered once by microwave to form a special small-scale hybrid complex structure, so that the giant dielectric constant and the dielectric constant external field adjustable characteristic are generated.
2. The method for preparing a lead-free ferroelectric ceramic material according to claim 1, comprising the steps of:
(1) according to BaTi0.90Sn0.10O3Respectively weighing and analyzing pure raw material BaCO according to the stoichiometric ratio3、SnO2And TiO2Putting the mixture into a ball milling tank, taking zirconia as a milling ball and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 24 hours, separating the milling ball, drying the raw materials at 60 ℃, and then performing heat preservation in a high-alumina crucible at 1200 ℃ for 2 hours to synthesize BaTi in advance0.90Sn0.10O3Powder;
(2) according to Ca2LaMn2O7Respectively weighing CaCO as a raw material for analysis3、La2O3And MnO2Is put into a ball millIn a pot, zirconium oxide is used as a grinding ball and absolute ethyl alcohol is used as a ball milling medium, the mixture is fully mixed and ball milled for 24 hours, the grinding ball is separated, the raw materials are dried at 60 ℃, and then the mixture is preserved in a high-alumina crucible at 1300 ℃ for 2 hours to synthesize Ca in advance2LaMn2O7Powder;
(3) the synthesized BaTi0.90Sn0.10O3Powder and Ca2LaMn2O7Powder according to (1-x)BaTi0.90Sn0.10O3- xCa2LaMn2O7Proportioning in a stoichiometric mode;
(4) ball-milling the raw materials prepared in the step (3) for 15 hours by using absolute ethyl alcohol as a medium, drying, adding 5% of PVA (polyvinyl alcohol) for granulation, and carrying out cold isostatic pressing at 150 Mpa;
(5) rapidly sintering the raw materials formed in the step (4) by adopting microwave, preserving heat for 30 minutes at 1400 ℃, and sintering into porcelain; the sintered sample is processed into a sheet with smooth two sides, and the two-side silver-plated electrode is prepared into the lead-free ferroelectric ceramic material with giant dielectric constant and electric regulation characteristics.
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| SU658114A1 (en) * | 1977-09-07 | 1979-04-25 | Ponomarenko Vasilij D | Heat-compensated glass-ceramic material |
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| SU658114A1 (en) * | 1977-09-07 | 1979-04-25 | Ponomarenko Vasilij D | Heat-compensated glass-ceramic material |
| CN102176509A (en) * | 2011-01-14 | 2011-09-07 | 西南交通大学 | Composite phase perovskite manganese oxide magnetoresistance material using metal adhesive |
| CN104692800A (en) * | 2015-02-04 | 2015-06-10 | 桂林理工大学 | Temperature-stable lead-free giant dielectric constant ceramic material |
| CN107151138A (en) * | 2017-05-02 | 2017-09-12 | 桂林电子科技大学 | Low-loss extra-high voltage performance lead-free piezoceramic material and preparation method thereof |
| CN107500753A (en) * | 2017-09-06 | 2017-12-22 | 天津大学 | A kind of low-loss titanium barium stannate dielectric material |
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| Title |
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| "La4/3 Ca5/3 Mn2 O7 的结构、电输运及磁性质研究";刘莉 等;《低温物理学报》;20070531;第29卷(第2期);第90-93页 * |
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Application publication date: 20181023 Assignee: Guilin Sensing Material Technology Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2022450000575 Denomination of invention: A lead-free ferroelectric ceramic material with giant dielectric constant and electrical modulation characteristics and its preparation method Granted publication date: 20210105 License type: Common License Record date: 20221230 |
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